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Automated online pretreatment and cleanup recycle coupled with high‐performance liquid chromatography‐mass spectrometry for determination of deca‐bromodiphenyl ether in human serum
Authors:Xuexia Lin  Hai‐Fang Li  Xiangwei He  Yuki Hashi  Jin‐Ming Lin  Zhihua Wang
Affiliation:1. State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, , Beijing, China;2. Beijing Key Laboratory of Analytical Methods and Instrumentation, Department of Chemistry, Tsinghua University, , Beijing, China;3. Shimadzu Corporation, Global COE for Application & Technical Development, , Shanghai, China
Abstract:Automated online SPE‐HPLC‐MS was established for the determination of deca‐bromodiphenyl ether in human serum. The online SPE with large volume injection was utilized to enhance the sensitivity. Online SPE with dilution line greatly decreased matrices effect, which enabled serum samples to be injected directly into pre‐column. Washing line was designed for the system to solve the serious residual phenomenon and reduce the risk of sample wastage and contamination. Under the optimized conditions, the linear of the method was in the range 0.1–10 ng/mL with the LOD of 0.026 ng/mL. The recoveries of serum samples spiked with deca‐bromodiphenyl ether at 0.5 ng/mL was in the range from 83.30 to 102.7% with RSD in interday less than 8.67%. The satisfactory results demonstrated that the method of online sample pretreatment and cleanup recycle were reliable for human serum analysis.
Keywords:DBDE  High‐performance liquid chromatography  Mass spectrometry  Online solid‐phase extraction
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